CN105788758A - Method for preparing low-cost lead-free photosensitive electrode paste - Google Patents
Method for preparing low-cost lead-free photosensitive electrode paste Download PDFInfo
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- CN105788758A CN105788758A CN201610157560.7A CN201610157560A CN105788758A CN 105788758 A CN105788758 A CN 105788758A CN 201610157560 A CN201610157560 A CN 201610157560A CN 105788758 A CN105788758 A CN 105788758A
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- lead
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- silver
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002003 electrode paste Substances 0.000 title abstract 7
- 239000000843 powder Substances 0.000 claims abstract description 39
- 239000011521 glass Substances 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011267 electrode slurry Substances 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 239000005331 crown glasses (windows) Substances 0.000 claims description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 15
- 239000010930 yellow gold Substances 0.000 claims description 15
- 229910001097 yellow gold Inorganic materials 0.000 claims description 15
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000000016 photochemical curing Methods 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- 229910052810 boron oxide Inorganic materials 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229920000609 methyl cellulose Polymers 0.000 claims description 6
- 239000001923 methylcellulose Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- MOWNZPNSYMGTMD-UHFFFAOYSA-N oxidoboron Chemical class O=[B] MOWNZPNSYMGTMD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 239000000440 bentonite Substances 0.000 abstract description 2
- 229910000278 bentonite Inorganic materials 0.000 abstract description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 abstract description 2
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 239000001913 cellulose Substances 0.000 abstract description 2
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000002562 thickening agent Substances 0.000 abstract description 2
- 239000013008 thixotropic agent Substances 0.000 abstract description 2
- 229910000881 Cu alloy Inorganic materials 0.000 abstract 2
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 abstract 2
- 241000779819 Syncarpia glomulifera Species 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000001739 pinus spp. Substances 0.000 abstract 1
- 229940036248 turpentine Drugs 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to a method for preparing low-cost lead-free photosensitive electrode paste, and belongs to the field of electronic materials. The method comprises the following steps: preparing carrier resin with methacrylic acid as a raw material, preparing silver-copper alloy powder and lead-free glass slags, grinding the components in a three-roller machine together with a turpentine solvent, a cellulose thickener and a bentonite thixotropic agent to obtain the low-cost lead-free photosensitive electrode paste. According to the photosensitive electrode paste prepared by the method provided by the invention, the silver-copper alloy powder replaces the silver powder to serve as a conductive phase, and copper replaces the silver to solve the problem of high production cost resulting from the traditional electrode paste employs the silver powder as the conductive phase, on the condition of not obviously reducing the electrical conductivity, meanwhile, the lead-free glass replaces the lead-containing glass to serve as an adhesive, which compensates the shortcomings that the lead contained in the traditional electrode paste is liable to generate damage to the environment and the human body, so the novel lead-free photosensitive electrode paste is low in cost, environmental friendly and is suitable for large scale production.
Description
Technical field
The preparation method that the present invention relates to the unleaded photonasty electrode slurry of a kind of low cost, belongs to field of electronic materials.
Background technology
Electronic industrial products is both closely bound up with national life, from mobile phone to TV, has the figure of electronic industrial products everywhere, and it is again a kind of embodiment of overall national strength, and from military project to aviation, the application of electronic industrial products is ubiquitous.Thus it is known that the scale of electronics industry development, it is that overall national strength develops whether powerful important symbol, the process of national economic development is occupied considerable status.And as one of the basic material of electronic industrial products, the research and development of electric slurry have had been subjected to increasing attention.Electric slurry is as the extremely important ingredient of electronic industrial material, and its quality and performance directly determine quality and the performance of final products.The key technology of electronic industrial products updates very fast, to the electric slurry as electronic industrial products important component part, it is proposed that update higher requirement.
Electric slurry, as the basic material of electronics and information industry, according to different in kind, has different sorting techniques.Thick-film electronic slurry is then an electric slurry commercially modal kind, constantly updates along with the development of electronics and information industry always.Thick-film electronic slurry, mainly based on metallic conductor slurry, mainly includes monomer slurry, alloy pulp, organic metal slurry and photonasty electrode slurry.
Photonasty electrode slurry is compared the maximum advantage of traditional electric slurry and is in that it both can be printed by screen printing technique large area, the electrode line of precision can be made again by photoetching technique, the electrode line width prepared by photonasty electrode slurry method can reach 30～50 μm, even and traditional silk-screen printing technique is the most harsh when, the electrode line width made is minimum also can only achieve 80 μm, therefore in current electronics and information industry to integrated, precise treatment, during the direction of miniaturization is developed, the development of photonasty electrode slurry seems and is even more important.
Summary of the invention
The technical problem that present invention mainly solves: compare the maximum advantage of traditional electric slurry for current photonasty electrode slurry and be in that it both can be printed by screen printing technique large area, the electrode line of precision can be made again by photoetching technique, more meet current electronics and information industry to integrated, precise treatment, the trend of miniaturization, but common photonasty electrode material is many using argentum powder as conductive phase, lead bearing glass powder makes binding agent, wherein argentum powder virtually adds the production cost of slurry as noble metal, constrain its large-scale production, and lead bearing glass in process of production can to environment, the defect that human body is damaged, the preparation method providing the unleaded photonasty electrode slurry of a kind of low cost.The method prepares vector resin with methacrylic acid for raw material, and make yellow gold powder and crown glass slag by oneself, it is aided with Oleum Terebinthinae solvent, cellulose thickener, namely bentonite thixotropic agent etc. obtains the unleaded photonasty electrode slurry of low cost after three-roller grinds, the photonasty electrode slurry that the present invention prepares replaces argentum powder to make conductive phase with yellow gold powder, replace part silver when significantly reducing electric conductivity with copper, solve the deficiency that traditional electrode slurry causes production cost high with argentum powder as conductive phase, crown glass replaces lead bearing glass as binding agent simultaneously, compensate for again the leaded deficiency easily environment and human body damaged in traditional electrode slurry, it it is a kind of low cost, the novel photoactive electrode slurry of environmental protection, it is suitable for large-scale production.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) measuring 200～300mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 85～95 DEG C；
(2) it is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 100～150mL volume ratio again after reaching bath temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 40～50min, to dropwise follow-up continuous insulation reaction 2～3h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；
(3) 200～300mL concentration is 0.3mol/L silver nitrate solution and 100～150mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 200～300mL mass concentration is 0.5～0.8% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 20～30min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 6000～7000r/min after terminating, standby after drying；
(4) mark meter loads in silica crucible after weighing 60～70 parts of bismuth oxide, 5～10 parts of silicon dioxide, 7～15 parts of boron oxides, 3～5 parts of zinc oxide, 2～3 parts of aluminium oxidies and 1～3 part of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1200～1300 DEG C of high temperature melting 1～3h, the vitreous humour obtained is poured into rapidly in the frozen water of 4～6 DEG C and carry out cold quenching, obtain crown glass slag；
(5) for 1:2:1,100g stainless steel ball-milling pearl is loaded in planetary ball mill by ball feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 1～2h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 105～110 DEG C after sieving；
(6) weigh 100～200g vector resin powder, 400～500mL Oleum Terebinthinae, 20～30g methylcellulose powder, 10～15g organobentonite and 1～2g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 20～30min at 70～80 DEG C, obtains dense thick organic carrier；
(7) measure the above-mentioned prepared organic carrier of 300～400mL and 20～30mL acrylic acid methyl ester. and 0.5～1g diaryl group iodized salt loads in planetary agitator, after stirring mixing 20～30min with 300～400r/min rotating speed, obtain organic carrier photocuring system mixture；
(8) in 300～350mL above-mentioned organic carrier photocuring system mixture, yellow gold powder standby for 10～15g and 30～40g lead-free glass powder are continuously added, pour in three-roll grinder after continuing stirring 60～80min and be ground, until slurry fineness stops grinding when reaching 3～5 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
The concrete application process of the present invention: the unleaded photonasty electrode slurry of low cost that the present invention prepares can be used for manufacturing the electrotechnical elements such as the electronic component such as capacitor, potentiometer and high voltagehigh frequency porcelain piece, the electrode line width prepared by photonasty electrode slurry of the present invention reaches 30～40 μm, it is that traditional electrode slurry can prepare less than the 1/2 of the thinnest width, meets the purpose of current electronics and information industry precise treatment, miniaturization.
The invention has the beneficial effects as follows:
(1) the photonasty electrode slurry that the present invention prepares replaces argentum powder to make conductive phase with yellow gold powder, replaces part silver when significantly reducing electric conductivity with copper, solves the deficiency that traditional electrode slurry causes production cost high with argentum powder as conductive phase；
(2) the photonasty electrode slurry that the present invention prepares replaces lead bearing glass as binding agent using crown glass, compensate for again the leaded deficiency easily environment and human body damaged in traditional electrode slurry, it is the novel photoactive electrode slurry of a kind of low cost, environmental protection, is suitable for large-scale production.
Detailed description of the invention
Measuring 200～300mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 85～95 DEG C；It is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 100～150mL volume ratio again after reaching bath temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 40～50min, to dropwise follow-up continuous insulation reaction 2～3h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；200～300mL concentration is 0.3mol/L silver nitrate solution and 100～150mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 200～300mL mass concentration is 0.5～0.8% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 20～30min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 6000～7000r/min after terminating, standby after drying；Mark meter loads in silica crucible after weighing 60～70 parts of bismuth oxide, 5～10 parts of silicon dioxide, 7～15 parts of boron oxides, 3～5 parts of zinc oxide, 2～3 parts of aluminium oxidies and 1～3 part of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1200～1300 DEG C of high temperature melting 1～3h, the vitreous humour obtained is poured into rapidly in the frozen water of 4～6 DEG C and carry out cold quenching, obtain crown glass slag；By ball, 100g stainless steel ball-milling pearl is loaded in planetary ball mill for 1:2:1 by feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 1～2h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 105～110 DEG C after sieving；Weigh 100～200g vector resin powder, 400～500mL Oleum Terebinthinae, 20～30g methylcellulose powder, 10～15g organobentonite and 1～2g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 20～30min at 70～80 DEG C, obtains dense thick organic carrier；Measure the above-mentioned prepared organic carrier of 300～400mL and 20～30mL acrylic acid methyl ester. and 0.5～1g diaryl group iodized salt loads in planetary agitator, after stirring mixing 20～30min with 300～400r/min rotating speed, obtain organic carrier photocuring system mixture；Yellow gold powder standby for 10～15g and 30～40g lead-free glass powder is continuously added in 300～350mL above-mentioned organic carrier photocuring system mixture, pour in three-roll grinder after continuing stirring 60～80min and be ground, until slurry fineness stops grinding when reaching 3～5 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
Example 1
Measuring 200mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 85 DEG C；It is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 100mL volume ratio again after reaching bath temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 40min, to dropwise follow-up continuous insulation reaction 2h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；200mL concentration is 0.3mol/L silver nitrate solution and 100mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 200mL mass concentration is 0.5% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 20min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 6000r/min after terminating, standby after drying；Mark meter loads in silica crucible after weighing 60 parts of bismuth oxide, 5 parts of silicon dioxide, 7 parts of boron oxides, 3 parts of zinc oxide, 2 parts of aluminium oxidies and 1 part of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1200 DEG C of high temperature melting 1h, the vitreous humour obtained is poured into rapidly in the frozen water of 4 DEG C and carry out cold quenching, obtain crown glass slag；By ball, 100g stainless steel ball-milling pearl is loaded in planetary ball mill for 1:2:1 by feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 1h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 105 DEG C after sieving；Weigh 100g vector resin powder, 400mL Oleum Terebinthinae, 20g methylcellulose powder, 10g organobentonite and 1g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 20min at 70 DEG C, obtain dense thick organic carrier；Measure the above-mentioned prepared organic carrier of 300mL and 20mL acrylic acid methyl ester. and 0.5g diaryl group iodized salt loads in planetary agitator, to obtain organic carrier photocuring system mixture after 300r/min rotating speed stirring mixing 20min；Yellow gold powder standby for 10g and 30g lead-free glass powder is continuously added in 300mL above-mentioned organic carrier photocuring system mixture, pour in three-roll grinder after continuing stirring 60min and be ground, until slurry fineness stops grinding when reaching 3 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
The concrete application process of the present invention: the unleaded photonasty electrode slurry of low cost that the present invention prepares can be used for manufacturing the electrotechnical elements such as the electronic component such as capacitor, potentiometer and high voltagehigh frequency porcelain piece, the electrode line width prepared by photonasty electrode slurry of the present invention reaches 30 μm, it is that traditional electrode slurry prepares the 3/8 of the thinnest width, meets the purpose of current electronics and information industry precise treatment, miniaturization.
Example 2
Measuring 250mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 90 DEG C；It is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 125mL volume ratio again after reaching bath temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 45min, to dropwise follow-up continuous insulation reaction 3h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；250mL concentration is 0.3mol/L silver nitrate solution and 130mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 250mL mass concentration is 0.7% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 25min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 6500r/min after terminating, standby after drying；Mark meter loads in silica crucible after weighing 65 parts of bismuth oxide, 8 parts of silicon dioxide, 13 parts of boron oxides, 4 parts of zinc oxide, 2 parts of aluminium oxidies and 2 parts of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1250 DEG C of high temperature melting 2h, the vitreous humour obtained is poured into rapidly in the frozen water of 5 DEG C and carry out cold quenching, obtain crown glass slag；By ball, 100g stainless steel ball-milling pearl is loaded in planetary ball mill for 1:2:1 by feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 1h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 108 DEG C after sieving；Weigh 150g vector resin powder, 450mL Oleum Terebinthinae, 25g methylcellulose powder, 13g organobentonite and 1g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 25min at 75 DEG C, obtain dense thick organic carrier；Measure the above-mentioned prepared organic carrier of 350mL and 25mL acrylic acid methyl ester. and 0.8g diaryl group iodized salt loads in planetary agitator, to obtain organic carrier photocuring system mixture after 400r/min rotating speed stirring mixing 30min；Yellow gold powder standby for 13g and 35g lead-free glass powder is continuously added in 330mL above-mentioned organic carrier photocuring system mixture, pour in three-roll grinder after continuing stirring 70min and be ground, until slurry fineness stops grinding when reaching 4 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
The concrete application process of the present invention: the unleaded photonasty electrode slurry of low cost that the present invention prepares can be used for manufacturing the electrotechnical elements such as the electronic component such as capacitor, potentiometer and high voltagehigh frequency porcelain piece, the electrode line width prepared by photonasty electrode slurry of the present invention reaches 35 μm, it is that traditional electrode slurry prepares the 7/16 of the thinnest width, meets the purpose of current electronics and information industry precise treatment, miniaturization.
Example 3
Measuring 300mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 95 DEG C；It is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 150mL volume ratio again after reaching bath temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 50min, to dropwise follow-up continuous insulation reaction 3h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；300mL concentration is 0.3mol/L silver nitrate solution and 150mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 300mL mass concentration is 0.8% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 30min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 7000r/min after terminating, standby after drying；Mark meter loads in silica crucible after weighing 70 parts of bismuth oxide, 10 parts of silicon dioxide, 15 parts of boron oxides, 5 parts of zinc oxide, 3 parts of aluminium oxidies and 3 parts of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1300 DEG C of high temperature melting 3h, the vitreous humour obtained is poured into rapidly in the frozen water of 6 DEG C and carry out cold quenching, obtain crown glass slag；By ball, 100g stainless steel ball-milling pearl is loaded in planetary ball mill for 1:2:1 by feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 2h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 110 DEG C after sieving；Weigh 200g vector resin powder, 500mL Oleum Terebinthinae, 30g methylcellulose powder, 15g organobentonite and 2g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 30min at 80 DEG C, obtain dense thick organic carrier；Measure the above-mentioned prepared organic carrier of 400mL and 30mL acrylic acid methyl ester. and 1g diaryl group iodized salt loads in planetary agitator, to obtain organic carrier photocuring system mixture after 400r/min rotating speed stirring mixing 30min；Yellow gold powder standby for 15g and 40g lead-free glass powder is continuously added in 350mL above-mentioned organic carrier photocuring system mixture, pour in three-roll grinder after continuing stirring 80min and be ground, until slurry fineness stops grinding when reaching 5 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
The concrete application process of the present invention: the unleaded photonasty electrode slurry of low cost that the present invention prepares can be used for manufacturing the electrotechnical elements such as the electronic component such as capacitor, potentiometer and high voltagehigh frequency porcelain piece, the electrode line width prepared by photonasty electrode slurry of the present invention reaches 40 μm, it is that traditional electrode slurry prepares the 1/2 of the thinnest width, meets the purpose of current electronics and information industry precise treatment, miniaturization.
Claims (1)
1. the preparation method of the unleaded photonasty electrode slurry of low cost, it is characterised in that concrete preparation process is:
(1) measuring 200～300mL butanone, to pour volume into be in the 500mL there-necked flask with agitator, passage and Dropping funnel, passage drain in bottle air to nitrogen logical in flask and move in water-bath, being heated to 85～95 DEG C；
(2) it is that the methacrylic acid of 2:2:1, methyl methacrylate and azodiisobutyronitrile mixed liquor load Dropping funnel by 100～150mL volume ratio again after reaching predetermined temperature, start agitator and be slowly added dropwise mixed liquor in the process of stirring, control rate of addition to make in its 40～50min, to dropwise follow-up continuous insulation reaction 2～3h, obtain transparent pastel to pulverize after vacuum drying, obtain vector resin powder；
(3) 200～300mL concentration is 0.3mol/L silver nitrate solution and 100～150mL concentration is load in 1L beaker after 0.5mol/L copper nitrate solution mix homogeneously, continuously adding 200～300mL mass concentration is 0.5～0.8% hydrazine hydrate solution, it is placed on shaking table by beaker oscillating reactions 20～30min again, reaction is centrifugally separating to obtain yellow gold powder precipitation with horizontal centrifuge with 6000～7000r/min after terminating, standby after drying；
(4) mark meter loads in silica crucible after weighing 60～70 parts of bismuth oxide, 5～10 parts of silicon dioxide, 7～15 parts of boron oxides, 3～5 parts of zinc oxide, 2～3 parts of aluminium oxidies and 1～3 part of calcium oxide mix homogeneously by weight, with tube type resistance furnace with 1200～1300 DEG C of high temperature melting 1～3h, the vitreous humour obtained is poured into rapidly in the frozen water of 4～6 DEG C and carry out cold quenching, obtain crown glass slag；
(5) for 1:2:1,100g stainless steel ball-milling pearl is loaded in planetary ball mill by ball feed liquid proportions together with corresponding crown glass slag and dehydrated alcohol, filter and cross 200 mesh standard sieves after wet ball grinding 1～2h, then glass dust is put into baking oven and is drying to obtain lead-free glass powder at 105～110 DEG C after sieving；
(6) weigh 100～200g vector resin powder, 400～500mL Oleum Terebinthinae, 20～30g methylcellulose powder, 10～15g organobentonite and 1～2g3-aminopropyl triethoxysilane and pour in 1L round-bottomed flask, ultrasonic disperse 20～30min at 70～80 DEG C, obtains dense thick organic carrier；
(7) measure the above-mentioned prepared organic carrier of 300～400mL and 20～30mL acrylic acid methyl ester. and 0.5～1g diaryl group iodized salt loads in planetary agitator, after stirring mixing 20～30min with 300～400r/min rotating speed, obtain organic carrier photocuring system mixture；
(8) in 300～350mL above-mentioned organic carrier photocuring system mixture, yellow gold powder standby for 10～15g and 30～40g lead-free glass powder are continuously added, pour in three-roll grinder after continuing stirring 60～80min and be ground, until slurry fineness stops grinding when reaching 3～5 μm, after discharging tinning, namely obtain the unleaded photonasty electrode slurry of a kind of low cost.
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| CN107742544A (en) * | 2017-09-19 | 2018-02-27 | 常州市丰瑞电子有限公司 | A kind of photosensitive electrode slurry and preparation method thereof |
| CN108766619A (en) * | 2018-05-28 | 2018-11-06 | 原晋波 | A kind of electronic component electrode slurry and preparation method thereof |
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